CN104833675A - Determination method of content of calcium oxide in iron ore - Google Patents
Determination method of content of calcium oxide in iron ore Download PDFInfo
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- CN104833675A CN104833675A CN201510260002.9A CN201510260002A CN104833675A CN 104833675 A CN104833675 A CN 104833675A CN 201510260002 A CN201510260002 A CN 201510260002A CN 104833675 A CN104833675 A CN 104833675A
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- iron ore
- sample
- calcium oxide
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- concentration
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 37
- 239000000292 calcium oxide Substances 0.000 title claims abstract description 30
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title claims abstract description 30
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title abstract description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 34
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000012086 standard solution Substances 0.000 claims abstract description 16
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims abstract description 14
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000011575 calcium Substances 0.000 claims abstract description 14
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 14
- 150000003839 salts Chemical class 0.000 claims abstract description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000012085 test solution Substances 0.000 claims abstract description 9
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229960002378 oftasceine Drugs 0.000 claims abstract description 8
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims abstract description 7
- 235000019341 magnesium sulphate Nutrition 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 238000003556 assay Methods 0.000 claims description 11
- 230000008034 disappearance Effects 0.000 claims description 5
- 229910052720 vanadium Inorganic materials 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- 238000007865 diluting Methods 0.000 abstract 1
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical compound O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 11
- 229910000831 Steel Inorganic materials 0.000 description 10
- 239000010959 steel Substances 0.000 description 10
- 238000005259 measurement Methods 0.000 description 7
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 229910000805 Pig iron Inorganic materials 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910000851 Alloy steel Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000010306 acid treatment Methods 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000010962 carbon steel Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- VFNGKCDDZUSWLR-UHFFFAOYSA-N disulfuric acid Chemical compound OS(=O)(=O)OS(O)(=O)=O VFNGKCDDZUSWLR-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052595 hematite Inorganic materials 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 229910001021 Ferroalloy Inorganic materials 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 239000008896 Opium Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 241001417490 Sillaginidae Species 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 229920001617 Vinyon Polymers 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- ZCHPOKZMTJTNHI-UHFFFAOYSA-L barium(2+);sulfonatooxy sulfate Chemical compound [Ba+2].[O-]S(=O)(=O)OOS([O-])(=O)=O ZCHPOKZMTJTNHI-UHFFFAOYSA-L 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229910052635 ferrosilite Inorganic materials 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229960001027 opium Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000013215 result calculation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000005477 standard model Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a determination method of content of calcium oxide in iron ore. The method comprises the following steps: adding an iron ore sample which is m in mass to a polytetrafluoroethylene beaker while not adding the sample to another beaker as blank control, respectively adding hydrochloric acid, hydrofluoric acid and nitric acid to dissolve the sample, then adding sulfuric aid until smoke comes out, taking down when the sample is in the form of wet salt, cooling, respectively adding hydrochloric acid, heating and dissolving salts, respectively transferring test solutions to large-volume flasks, diluting to set scales and setting constant volumes, respectively taking quantitative solutions from the solutions with the constant volumes, adding into the beakers, respectively adding triethanolamine, water and hydroxylamine hydrochloride, adding potassium hydroxide solution to keep pH to be no less than 12, adding some drops of magnesium sulfate and proper amount of a calcein indicator, titrating with an EDTA standard solution which is C in concentration until fluorescent green disappears, and respectively recording volumes as V and V0, thus obtaining calcium content as follows: WCaO%=C (V-V0)MCaO100/mK*100.
Description
Technical field
The present invention relates to analysis of iron ore field, be specifically related to the assay method of calcium oxide content in a kind of volumetric determination iron ore.
Background technology
Iron ore is mainly used in steel and iron industry, smelts the different pig iron (carbon content is generally more than 2%) of carbon content and steel (carbon content is generally below 2%).The pig iron is divided into conversion pig, foundry iron, alloy pig iron by purposes difference usually.Steel is divided into carbon steel, alloy steel by component difference.Alloy steel is on the basis of carbon steel, and have a mind to add the steel of one or more appropriate elements for improving or obtain some performance, the element kind added in steel is a lot, mainly contains chromium, manganese, vanadium, titanium, nickel, molybdenum, silicon.In addition, iron ore is also for making the catalyzer (pure magnetic iron ore deposit) of synthetic ammonia, natural minerals pigment (haematite, specularite, limonite), feed addictive (magnetic iron ore, haematite, limonite) and famous and precious remedies (magnetite) etc., but consumption is little.Steel product is widely used in each department of national economy and people's lives various aspects, is the necessary stock of social production and public life.Since 19th century invention in mid-term converting process progressively forms the large production of steel and iron industry, iron and steel is most important structured material always, in national economy, occupy epochmaking status, be the mainstay industry of social development, is the metal material that modernization industry is most important and application is maximum.So, people often using the output of steel, steel, kind, quality as the important symbol of measurement National Industrial, agricultural, national defence and scientific technological advance level.
Ironmaking iron ore, can be divided into by the potential of hydrogen of slag making component:
Alkalescence ore (CaO+MgO)/(SiO
2+ Al
2o
3) > 1.2;
Self-fluxing ore (CaO+MgO)/(SiO
2+ Al
2o
3)=0.8 ~ 1.2;
Half self-fluxing ore (CaO+MgO)/(SiO
2+ Al
2o
3)=0.5 ~ 0.8;
Acid drift (CaO+MgO)/(SiO
2+ Al
2o
3) < 0.5.
Acid drift, self-fluxing ore, half self-fluxing ore and alkaline ore can be divided into according to iron ore slag forming constituents content.
CaO+MgO/SiO
2+ Al
2o
3=0.8 ~ 1.2 is autolyzed ore.
According to (CaO+MgO)/(SiO
2+ Al
2o
3) ratio determination ore type, when ratio is greater than 1.2 for alkaline ore; Ratio be 0.8-1.2 for self-fluxing ore; Ratio be 0.5-0.8 be half self-fluxing ore.When ferrosilite is greater than 2-3%, the full iron requirement of corresponding raising.
When geologic prospecting, to providing the ore directly entering stove and use, all slag making component concentration to be found out.As MgO, Al in ore
2o
3time all very low, CaO/SiO can be adopted
2determine potential of hydrogen.
Therefore the Accurate Determining carrying out calcium oxide in iron ore is significant.
The method measuring calcium oxide in iron ore has instrumental analysis and chemical analysis two kinds.Large enterprise adopts large-scale instrument analysis mostly, but cost is high, and for small business, chemical analysis method embodies its advantage more, namely convenient, fast.Chemical analysis iron ore oxidation calcium catalyst generally adopts platinum sheet half molten, and need demanganize, ammoniacal liquor is separated interference element, and operate more loaded down with trivial details, time-consuming, cost is high.This method sample, after vinyon beaker dissolves, does not need demanganize, does not carry out ammoniacal liquor and is separated interference element, directly shelter interference element when titration with triethanolamine, the separation not carrying out precipitating, filtration, washing.Substantially reduce analysis time, decrease loss, improve accuracy.Enhance productivity, reduce reagent consumption and cost of labor, method is easy to grasp and result precision is high, can apply aborning.Use equipment is simple, and analysis process is short, has feature accurately and rapidly, is suitable for calcium oxide determination and analysis in iron ore.
Summary of the invention
When measuring calcium content in iron ore in order to solve in existing method, the problem of length consuming time.The invention provides a kind of more fast, measure the method for calcium content in iron ore accurately and efficiently.
For reaching above-mentioned purpose, the assay method of calcium oxide content in a kind of iron ore of the present invention, comprises the following steps:
The iron ore sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add hydrochloric acid respectively, hydrofluorite, nitric acid dissolve sample, add sulfuric acid afterwards to smolder, treat that sample is wet salt shape, take off, after cooling, add hydrochloric acid heating for dissolving salt respectively, respectively test solution is transferred in Large Copacity bottle, be diluted to scale constant volume, after constant volume solution, divide and get volumetric soiutions in beaker, add triethanolamine successively respectively, water, oxammonium hydrochloride, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, meter lower volume is for being respectively V and V
0, obtaining calcium content is: W
caO%=C (V-V
0) M
caO100/m K × 100,
In formula: M
caO: the molal weight of calcium oxide, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V: sample consumes the volume of EDTA standard solution, mL;
V
0: the blank volume consuming EDTA standard solution, mL.
The concentration of wherein said hydrochloric acid and described hydrofluorite is respectively 65% and 40%.
Wherein on low temp. electric hot plate at 100 DEG C dissolved samples.
Wherein said sulfuric acid concentration is 5%.
Wherein said concentration of nitric acid is 67%.
Wherein said triethanolamine concentrations is 12%.
Wherein said potassium hydroxide solution concentration is 20%.
Wherein said Adlerika concentration is 0.5%.
The invention difference from existing technology is that the present invention achieves following technique effect:
1) fast, efficiently, low cost: the method substantially reduces operating process, has saved medicine, has reduced testing cost, improve production efficiency.
2) accurately, stable: adopt the result that this method measures, after demanganize, ammoniacal liquor is separated interference element twice, and both measurement results are the same.Ensure that measurement result is stablized, data are accurate.
Embodiment
Below in conjunction with embodiment, to above-mentioned being described in more detail with other technical characteristic and advantage of the present invention.
1. method summary: adopt hydrochloric acid (65%) in polytetrafluoroethylplastic plastic beaker, nitric acid (67%)-hydrofluorite (40%) dissolved samples, add sulfuric acid and smolder that (sulfuric acid has been smoldered 1-2 minute after opium, both sample was wet salt shape, the overlong time if sulfuric acid is smoldered, barium sulphate and calcium sulphate can generate barium persulfate and the persulfuric acid calcium later stage has added dissolving with hydrochloric acid not, can affect measurement result.In addition, in beaker, sample has black residue, and after residue treatment, measuring calcium in residue is zero.Therefore, can say that in sample, calcium dissolves completely after a series of acid treatment in early stage, so the later stage directly can measure calcium, unnecessaryly carry out residue treatment.) take off, after cooling, carefully add 5mL hydrochloric acid (65%) along wall of cup, heating for dissolving salt.Test solution is transferred in 250mL volumetric flask, be diluted to scale fixed molten, point getting 50mL solution in 250mL beaker, adding 50mL triethanolamine (12%) (must first add, be to first be sheltered by the interference element such as iron and aluminium), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), add several magnesium sulfate (0.5%), calcein is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.
2. reagent:
2.1 nitric acid (67%)
2.2 hydrofluorite (40%)
2.3 sulfuric acid (5%)
2.4 hydrochloric acid (65%)
2.5 oxammonium hydrochlorides (solid)
2.6 triethanolamines (12%)
2.7 potassium hydroxide aqueous solutions (20%)
2.8 calcein indicator: 1g calcein and 100g dry after sodium chloride porphyrize mix, be placed in port grinding bottle for subsequent use.
2.9EDTA standard solution C (EDTA)=0.01783mol/L
2.10 magnesium sulfate solutions (0.5%)
3. sampling and sample preparation: get sample preparation standard according to ferroalloy and carry out sample and produce.
4. sample weighting amount: take sample 0.2500g
5. analytical procedure:
Specimen test: take sample m0.2500g in polytetrafluoroethylene beaker, add 10mL hydrochloric acid (65%), add 10mL hydrofluorite (40%), at the upper dissolved samples of low temp. electric hot plate (100 DEG C), after sample major part is dissolved, add 5mL nitric acid (67%), add 20mL sulfuric acid (5%), continue to be heated to sulfuric acid to smolder, test solution is wet salt shape, (this walks key, test solution is that wet salt shape just takes off, the not too long time, otherwise, form indissoluble pyrosulfuric acid calcium and pyrosulfuric acid barium, to next step with dissolving with hydrochloric acid not, affect measurement result.In addition, in beaker, sample has black residue, and after residue treatment, measuring calcium in residue is zero.Therefore, can say that in sample, calcium dissolves completely after a series of acid treatment in early stage, so the later stage directly can measure calcium, unnecessaryly carry out residue treatment.) take off, after cooling, carefully add 5mL hydrochloric acid (65%) along wall of cup, heating for dissolving salt.Test solution is transferred in 250mL volumetric flask, be diluted to scale fixed molten, from 250mL volumetric flask, divide and get 50mL solution in 250mL beaker, add 50mL triethanolamine (12%) (must first add, to first the interference element such as iron and aluminium be sheltered), add 50mL water, add oxammonium hydrochloride a little (further masking action), add 30mL potassium hydroxide solution (20%) (buffer solution), add several magnesium sulfate (0.5%), calcein is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Meter lower volume V.
Blank test: in polytetrafluoroethylene beaker, add 10mL hydrochloric acid (65%), add 10mL hydrofluorite (40%), at the upper dissolved samples of low temp. electric hot plate (100 DEG C), add 5mL nitric acid (67%), add 20mL sulfuric acid (5%), continue to be heated to sulfuric acid and smolder, test solution is wet salt shape, take off, after cooling, carefully add 5mL hydrochloric acid (65%) along wall of cup, heating for dissolving salt.Test solution is transferred in 250mL volumetric flask, be diluted to scale fixed molten, from 250mL volumetric flask, divide and get 50mL solution in 250mL beaker, add 50mL triethanolamine (12%), add 50mL water, add oxammonium hydrochloride a little, add 30mL potassium hydroxide solution (20%), add several magnesium sulfate (0.5%), calcein is appropriate, and being titrated to fluorescence green disappearance with EDTA standard solution is terminal.Meter lower volume V
0.
6. Analysis result calculation:
W
CaO％＝C(V-V
0)M
CaO100/m K×100；
In formula: M (CaO): the molal weight (g/mol) of calcium oxide;
M: sample mass (g);
K: sample divides liquor ratio;
C:EDTA concentration of standard solution (mol/L);
V: sample consumes the volume (mL) of EDTA standard solution;
V0: the blank volume (mL consuming EDTA standard solution.
7. standard specimen analysis of control:
Accuracy is as shown in table 1:
Table 1 measures sample and standard model measured value
As can be seen from Table 1: data are accurate, and operating process is short, fast, efficient.
Precision is as shown in table 2:
Table 2 sample repetitive measurement value
As can be seen from Table 2: measurement result precision is good.
8. conclusion:
By this method, the content of calcium oxide in iron ore can be determined accurately.Substantially reduce the running time, reduce energy consumption.Make determination data accurately and reliably, application obtains good effect aborning.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (8)
1. the assay method of calcium oxide content in iron ore, is characterized in that comprising the following steps:
The iron ore sample that quality is m is added polytetrafluoroethylene beaker one, another does not add as blank, add hydrochloric acid respectively, hydrofluorite, nitric acid dissolve sample, add sulfuric acid afterwards to smolder, treat that sample is wet salt shape, take off, after cooling, add hydrochloric acid heating for dissolving salt respectively, respectively test solution is transferred in Large Copacity bottle, be diluted to scale constant volume, after constant volume solution, divide and get volumetric soiutions in beaker, add triethanolamine successively respectively, water, oxammonium hydrochloride, hydro-oxidation potassium solution keeps pH to be not less than 12, add several magnesium sulfate, calcein indicator is appropriate, being titrated to fluorescence green disappearance with the EDTA standard solution that concentration is C is terminal, meter lower volume is for being respectively V and V
0, obtaining calcium content is: W
caO%=C (V-V
0) M
caO100/mK × 100,
In formula: M
caO: the molal weight of calcium oxide, g/mol;
M: sample mass, g;
K: sample divides liquor ratio, the volumetric flask volume of the Large Copacity bottle of the volumetric soiutions got after K=/transfer to;
C:EDTA concentration of standard solution, mol/L;
V: sample consumes the volume of EDTA standard solution, mL;
V
0: the blank volume consuming EDTA standard solution, mL.
2. the assay method of calcium oxide content in iron ore according to claim 1, is characterized in that: the concentration of described hydrochloric acid and described hydrofluorite is respectively 65% and 40%.
3. the assay method of calcium oxide content in iron ore according to claim 1, is characterized in that: on low temp. electric hot plate at 100 DEG C dissolved samples.
4. the assay method of calcium oxide content in iron ore according to claim 1, is characterized in that: described sulfuric acid concentration is 5%.
5. the assay method of calcium oxide content in iron ore according to claim 1, is characterized in that: described concentration of nitric acid is 67%.
6. the assay method of calcium oxide content in iron ore according to claim 1, is characterized in that: described triethanolamine concentrations is 12%.
7. the assay method of calcium oxide content in iron ore according to claim 1, is characterized in that: described potassium hydroxide solution concentration is 20%.
8. the assay method of calcium oxide content in iron ore according to claim 1, is characterized in that: described Adlerika concentration is 0.5%.
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